Hydrochloric Acid → 5-Bromo-3-morpholinopyridin-2-ol
反応式
[Br:1][C:2]1[CH:3]=[C:4]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[C:5]([O:8]C)=[N:6][CH:7]=1.Cl>O1CCOCC1>[Br:1][C:2]1[CH:3]=[C:4]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[C:5](=[O:8])[NH:6][CH:7]=1参加物
4
反応条件
- 温度
- 100 °C
実験手順
To a solution of 4-(5-bromo-2-methoxypyridin-3-yl)morpholine (1.0 equiv.) in 1,4-dioxane (0.3 M) was added concentrated HCl (5 equiv.) and the solution was heated to 100° C. for 1 h. Upon cooling to room temperature, the solution was concentrated to dryness under vacuo, then dissolved in water and neutralized with solid sodium bicarbonate. The precipitate was filtered, washed with water and dried under vacuo to give 5-bromo-3-morpholinopyridin-2(1H)-one as a beige solid in 93% yield. LCMS m/z (M+H)=258.9/260.9, Rt=0.48 min.
後処理
- temperatureUpon cooling to room temperature
- concentrationthe solution was concentrated to dryness under vacuo
- dissolutiondissolved in water and neutralized with solid sodium bicarbonate
- filtrationThe precipitate was filtered
- washwashed with water
- customdried under vacuo
出典と根拠
- ORDレコード
- ord-c7c0573354f94c41b214776f9f52d15f
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09242969B2
反応ノート
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